CN101162779A - Preparation method of anode supporter of tube-type solid-oxide fuel battery - Google Patents
Preparation method of anode supporter of tube-type solid-oxide fuel battery Download PDFInfo
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- CN101162779A CN101162779A CNA2007100311053A CN200710031105A CN101162779A CN 101162779 A CN101162779 A CN 101162779A CN A2007100311053 A CNA2007100311053 A CN A2007100311053A CN 200710031105 A CN200710031105 A CN 200710031105A CN 101162779 A CN101162779 A CN 101162779A
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- Y02E60/30—Hydrogen technology
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention discloses a preparation method of a tube-type solid oxide fuel cell anode support body. The method comprises the preparation of a gypsum mold and the anode support body gained by injecting anode sizing agent to the gypsum mold; anode powders are gained through uniformly mixing NiO powders and YSZ powders with equal quality; water is added to the anode powders; anode injecting sizing agent is gained by planetary type ball milling; acacia as dispersant is added to the anode injecting sizing agent; the prepared anode injecting sizing agent is injected to the cavum of the gypsum mold and an anode layer is formed in the cavum of the gypsum mold; the anode tube is taken out and is presintered for 1 hour to 3 hours in the temperature between 800 DEG C and 1250 DEG C. The method can prepare anode support tubes with different shapes by changing the shape of the gypsum mold and can prepare NiO-YSZ compound anode support tubes. On the basis of the anode support tube prepared by the method of the invention, electrolytical membrane and the cathode are prepared on the anode support tube, and the battery has good output performance in a middle temperature zone (600 DEG C to 800 DEG C).
Description
Technical field:
The present invention relates to the preparation method of a kind of tubular anode support type Solid Oxide Fuel Cell and battery pack, be specifically related to the preparation method of anode supporter of small-sized conical tube type Solid Oxide Fuel Cell.
Background technology:
Solid Oxide Fuel Cell (SOFC) is a kind of novel Blast Furnace Top Gas Recovery Turbine Unit (TRT), and it is by anode, and electrolyte and negative electrode are formed.Anode and negative electrode are porous ceramic, are the places that electrochemical reaction takes place in the battery; Electrolyte is generally ceramic of compact, reduction reaction on negative electrode occurs in the dense electrolyte both sides respectively to fuel in oxidation reaction on the anode and oxidant, so just oxidation reaction and reduction reaction are kept apart from the space, cell reaction could produce net current; The oxonium ion or the proton that relate in the electrochemical reaction pass through electrolyte transport.
Application number is that 200510101487.3 Chinese invention patent discloses a kind of conical tube type positive electrode support solid oxide fuel cell monomer, as shown in Figure 1, comprise porous anode supporter, dense electrolyte film and porous cathode film, the dense electrolyte film is positioned at porous anode supporter outer, and the porous cathode film is positioned at dense electrolyte film outer; The porous anode supporter is that an end opening is big, the Taper Pipe shape that an end opening is little, and the outer rim of little openend is an arc; The dense electrolyte film covers porous anode supporter outer, comprises the arc outer rim of little openend; The dense electrolyte upper strata of cathode layer between the arc outer rim of the little openend of Taper Pipe and big openend end edge.This battery cell bulk is little, the battery power output big, making easily, is specially adapted to small-sized SOFC pile.The negative electrode of battery cell and the anode of another battery cell are connected in series by the mode of a Taper Pipe and another Taper Pipe socket easily, and sealing also is easier to realize.The porous anode supporter is mixed by 1: 1 weight ratio by the zirconic powder of nickel protoxide and stabillzed with yttrium, adopts the method preparation of injection moulding or injection forming.Prior art for preparing tubular anode supporter generally adopts extrusion moulding, and it is very convenient that this legal system is equipped with the elongated tubular anode support, but the Taper Pipe shape anode support that preparation can be connected in series mutually is difficult relatively.
The patent No. is that 99108725.9 Chinese invention patent discloses and adopts the gypsum mould grouting method to prepare the method for YSZ electrolyte thin wall tube; This method is in casting process, and the uniformity of slurry and suspension are very big to the quality influence of slip casting product.Because different types of solid particle all has sedimentation potential separately in water, preparation is even, and the multicomponent slip casting slurry that suspension is good is more difficult with respect to preparation one pack system slurry.Slip casting slurry in the above-mentioned patent is not seen the example that adopts slip casting to prepare nickel oxide (NiO)-YSZ Taper Pipe shape anode support so far by the preparation of single Y SZ pressed powder.
Summary of the invention:
The objective of the invention is to overcome the shortcoming of prior art, provide an a kind of end opening big, an end opening is little, mutually the preparation method of anode supporter of the small-sized conical tube type Solid Oxide Fuel Cell that is together in series of socket.
Purpose of the present invention is achieved through the following technical solutions:
The preparation method of anode supporter of tubular solid oxide fuel cell comprises the steps:
The preparation of a, plaster mold: 150～170 ℃ of parch 3～5 hours, be cooled to after the room temperature stand-by the anhydrous gypsum powder; The gypsum powder that parch is good with etc. the water of quality mix, stir, obtain gypsum slurry; Calcium plaster poured in the cylindrical metal mould fast solidify, slough off metal die, obtain being used for the plaster mold of injection forming anode support tube;
B, anode slurry is injected plaster mold obtain anode support: (1) will wait the NiO of quality and YSZ powder to obtain anode powder after evenly mixing; To add entry in the anode powder, planetary type ball-milling obtains anode slip casting slurry about 10～50 minutes, and the content of anode powder is 15～55wt% in the slurry; The gum arabic that adds 0.1～10wt% in the anode slurry is as dispersant; (2) anode slurry for preparing in (1) is injected the plaster mold cavity, water is absorbed by plaster mold in the slurry, forms an anode layer in the plaster mold cavity; After treating that anode tube in the plaster mold is dry and separate, with anode tube taking-up and 800～1250 ℃ of pre-burnings 1～3 hour in muffle furnace with the gypsum die body.
The present invention has following advantage with respect to prior art:
The first, prior art for preparing sheath supporter adopts extrusion moulding more, and this method prepares Taper Pipe shape anode support difficulty relatively.Slip casting can prepare the anode support tube of different profiles by the shape that changes gypsum mold, and Taper Pipe shape anode is an one;
The second, the existing example that the gypsum mould grouting method is applied to SOFC preparation technology is single pressed powder slip casting method, as injection forming YSZ film tube and injection forming lanthanum strontium manganate pipe; The present invention utilizes slip casting method can prepare NiO and YSZ composite anode stay pipe;
The 3rd, cell in the existing Taper Pipe concatenation type battery pack mostly is the electrolyte self-cradling type, the present invention changes the structure of cell into anode support type, prepare the compact YSZ dielectric film by infusion process at the anode-supported tube outer surface, significantly reduced the Ohmic resistance of YSZ dielectric film, improved the output characteristic of cell greatly, good output performance has been arranged at middle warm area (600～800 ℃).
Description of drawings:
Fig. 1 is a conical tube type positive electrode support solid oxide fuel cell series battery structural representation.1 is the porous anode supporter among the figure; The 2nd, the dense electrolyte film; The 3rd, the porous cathode film; The 4th, the portlet outer rim; The 5th, the large port outer rim; The 6th, connect and encapsulating material.
Fig. 2 a is the plaster mold metal die profile that the gypsum mould grouting method of forming prepares Taper Pipe shape anode support;
Fig. 2 b is the metal die profile that Fig. 2 a is full of calcium plaster;
Fig. 2 c is the plaster mold profile of Fig. 2 a;
Fig. 2 d is the gypsum mold profile that Fig. 2 c is full of anode slurry (NiO-YSZ-water);
Fig. 2 e is that the water in the anode slurry is blotted by gypsum mold, the Taper Pipe shape anode support that obtains.
Fig. 3 is the discharge curve and the power density curve of the cell for preparing of the present invention.Test is fuel with the wet hydrogen, and airborne oxygen is oxidant.
Embodiment:
Below in conjunction with drawings and Examples the present invention is further described, but the scope of protection of present invention is not limited to the scope that embodiment represents.
As shown in Figure 1, conical tube type positive electrode support solid oxide fuel cell monomer comprises porous anode supporter 1, dense electrolyte film 2 and porous cathode film 3, dense electrolyte film 2 is positioned at porous anode supporter 1 outer, and porous cathode film 3 is positioned at dense electrolyte film 2 outers; Porous anode supporter 1 is that an end opening is big, the Taper Pipe shape that an end opening is little, and the outer rim of little openend is an arc, promptly the portlet outer rim 4; Dense electrolyte film 2 covers porous anode supporter 1 outer, comprises the arc outer rim of little openend; Dense electrolyte 2 upper stratas of porous cathode film 3 between little openend outer rim 4 of Taper Pipe and big openend end edge 5.Cell is composed in series battery pack.The small end of first segment cell is a closed form, and second and third joint and even the later more small end of more piece cell are open state, guarantee that like this gas circuit of whole series battery is unimpeded, as shown in Figure 1.The small end of the second joint cell is inserted in the big end of first segment cell, and the junction is with silver conductive adhesive or the sealing of chromic lanthanum ceramics seal, sealing materials.Silver conductive adhesive or chromic acid lanthanum have following function: one, each cell is together in series, and work the effect of being connected and fixed; Its two, the cell junction is sealed, guarantee the air-tightness of series battery; The 3rd, between each cell of series battery, set up electrical connection.
Embodiment 1
When adopting the gypsum mould grouting method of forming to prepare porous anode supporter 1.The first step, plaster mold is by the cylindric aluminum alloy mould preparation shown in Fig. 2 a, and detailed process is: 150 ℃ of parch 5 hours, be cooled to after the room temperature stand-by the anhydrous gypsum powder; The gypsum powder that parch is good with etc. the water of quality mix, stir, obtain gypsum slurry; Calcium plaster is poured in the cylindrical metal mould shown in Fig. 2 a fast, and gypsum solidifies after 30 minutes, obtains the plaster mold that is used for the injection forming anode support tube shown in Fig. 2 c just slough off metal die;
Second step, anode slurry to be injected plaster mold obtain anode support, detailed process is:
(1) will wait the NiO of quality and YSZ powder evenly to obtain anode powder after the mixing; To add 85wt% water in the anode powder, planetary type ball-milling obtains anode slip casting slurry about 15 minutes, and the content of anode powder is 15wt% in the slurry; Add the gum arabic of 0.1wt% in the anode slurry as dispersant;
(2) shown in Fig. 2 d, use dropper that the anode slurry for preparing in (1) is injected the plaster mold cavity, water is absorbed by plaster mold in the slurry, forms an anode layer simultaneously in the plaster mold cavity, shown in Fig. 2 e; After treating that anode tube in the plaster mold is dry and separate, with anode tube taking-up and 800 ℃ of pre-burnings 3 hours in muffle furnace with the gypsum die body.So far, the anode support tube preparation is finished.This patent can not only prepare Taper Pipe shape anode support, also can prepare the equal diameter tubular support, is cylindrical shape as long as change conical plaster mold, just can obtain the anode support of different profiles.
Embodiment 2
When adopting the gypsum mould grouting method of forming to prepare porous anode supporter 1.The first step, plaster mold is by the cylindric aluminum alloy mould preparation shown in Fig. 2 a, and detailed process is: 160 ℃ of parch 4 hours, be cooled to after the room temperature stand-by the anhydrous gypsum powder; The gypsum powder that parch is good with etc. the water of quality mix, stir, obtain gypsum slurry, adding 3-5 with suction pipe drips pyridine as defoamer; As shown in Figure 2, calcium plaster is poured in the cylindrical metal mould shown in Fig. 2 a fast, gypsum solidifies after 30 minutes, obtains the plaster mold that is used for the injection forming anode support tube shown in Fig. 2 c just slough off metal die;
Second step, anode slurry to be injected plaster mold obtain anode support, detailed process is:
(1) will wait the NiO of quality and YSZ powder evenly to obtain anode powder after the mixing; To add 65wt% water in the anode powder, planetary type ball-milling obtains anode slip casting slurry about 30 minutes, and the content of anode powder is 35wt% in the slurry; Add the gum arabic of 5wt% in the anode slurry as dispersant;
(2) use dropper that the anode slurry for preparing in (1) is injected plaster mold cavity (Fig. 2 d), water is absorbed by plaster mold in the slurry, forms an anode layer simultaneously in the plaster mold cavity, shown in Fig. 2 e; After treating that anode tube in the plaster mold is dry and separate, with anode tube taking-up and 1000 ℃ of pre-burnings 2 hours in muffle furnace with the gypsum die body.So far, the anode support tube preparation is finished.This patent can not only prepare Taper Pipe shape anode support, also can prepare the equal diameter tubular support, as long as change the shape of plaster mold, just can obtain the anode support of different profiles.
Embodiment 3
When adopting the gypsum mould grouting method of forming to prepare porous anode supporter 1.The first step, plaster mold is by the cylindric aluminum alloy mould preparation shown in Fig. 2 a, and detailed process is: 170 ℃ of parch 3 hours, be cooled to after the room temperature stand-by the anhydrous gypsum powder; The gypsum powder that parch is good with etc. the water of quality mix, stir, obtain gypsum slurry, adding 3-5 with suction pipe drips absolute alcohol as defoamer; Calcium plaster is poured in the cylindrical metal mould shown in Fig. 2 a fast, and gypsum solidifies after 30 minutes, obtains the plaster mold that is used for the injection forming anode support tube shown in Fig. 2 c just slough off metal die;
Second step, anode slurry to be injected plaster mold obtain anode support, detailed process is:
(1) will wait the NiO of quality and YSZ powder evenly to obtain anode powder after the mixing; To add 45wt% water in the anode powder, planetary type ball-milling obtains anode slip casting slurry about 45 minutes, and the content of anode powder is 55wt% in the slurry; Add the gum arabic of 10wt% in the anode slurry as dispersant;
(2) use dropper that the anode slurry for preparing in (1) is injected the plaster mold cavity, as Fig. 2 d, water is absorbed by plaster mold in the slurry, forms an anode layer simultaneously in the plaster mold cavity, shown in Fig. 2 e; After treating that anode tube in the plaster mold is dry and separate, with anode tube taking-up and 1250 ℃ of pre-burnings 1 hour in muffle furnace with the gypsum die body.So far, the anode support tube preparation is finished.This patent can not only prepare Taper Pipe shape anode support, also can prepare the equal diameter tubular support, as long as change the shape of plaster mold, just can obtain the anode support of different profiles.
The preparation of dense electrolyte film 2: the preparation of anode-supported tube outer surface dielectric film adopts infusion process to carry out, detailed process is: (1) mixes 3g YSZ powder, 45g alcohol, 1.3g terpinol, 0.08g ethyl cellulose and 0.2g vegetable oil, obtains the YSZ slurry that is used to flood.Wherein, alcohol is solvent, and terpinol is a plasticizer, and ethyl cellulose is a binding agent, and vegetable oil is a dispersant; (2) anode support tube is immersed in the YSZ slurry, at the uniform velocity upwards lift anode tube after 3 seconds, make it to break away from YSZ slurry liquid level, so move in circles 5 times; (3) anode tube/YSZ dielectric film after will flooding is put into the high temperature muffle furnace and is carried out sintering, and concrete sintering schedule is: 300～500 ℃/3h of temperature-rise period; 500～900 ℃/4h; 900～1400 ℃/4h; 1400 ℃ of insulation 4h; 1400～900 ℃/4h of temperature-fall period; 900～500 ℃/3h; Naturally cool to room temperature with furnace temperature below 500 ℃.
The preparation of porous cathode film 3: adopt spread coating.Select La for use
0.7Sr
0.3MnO
3(60wt%)-YSZ (40wt%) is a composite cathode material.The little end opening of cathode layer edge and anode is all reserved suitable distance with big end opening, is short-circuited when preventing to carry out the cell series connection.At last sample was promptly got cell in 2 hours at 1200 ℃ of sintering.
The Taper Pipe shape anode supporting type solid oxide fuel cell that adopts the present embodiment preparation is carried out battery structure and electrochemical property test experiment, and its result is as follows:
The output performance of battery adopts four electrode method to measure, and filamentary silver is respectively as electric current and voltage lead.This test is a fuel with the hydrogen of saturated vapor under the room temperature, the output performance of battery is tested as oxidant with free-pouring air.As can be seen from Figure 6, this battery maximum power density in the time of 850 ℃ has reached 1.15W/cm
2When the work of the middle warm area below 800 ℃, the power output of battery is still considerable, and for example, power density is respectively 0.47W/cm when 750 ℃ and 700 ℃
2And 0.26W/cm
2Above test result shows that employing the inventive method has successfully prepared small-sized tubular type anode supporting type solid oxide fuel cell, and it can and can obtain desirable output characteristic in the middle warm area operation below 800 ℃.
Claims (6)
1. the preparation method of anode supporter of tubular solid oxide fuel cell is characterized in that comprising the steps:
The preparation of a, plaster mold: with the anhydrous gypsum powder 150～170 ℃ of parch 3～5 hours, be cooled to room temperature after; The gypsum powder that parch is good with etc. the water of quality mix, stir, obtain gypsum slurry; Calcium plaster poured in the metal die fast solidify, slough off metal die, obtain being used for the plaster mold of injection forming anode support tube;
B, anode slurry is injected plaster mold obtain anode support: (1) will wait the NiO of quality and YSZ powder to obtain anode powder after evenly mixing; Add entry in anode powder, planetary type ball-milling obtains anode slip casting slurry about 10～50 minutes, and the content of anode powder is 15～55wt% in the slurry; The gum arabic that adds 0.1～10wt% in the anode slurry is as dispersant; (2) anode slurry for preparing is injected the plaster mold cavity, water is absorbed by plaster mold in the slurry, forms an anode layer in the plaster mold cavity; After treating that anode tube in the plaster mold is dry and separate, with anode tube taking-up and pre-burning 1～3 hour under 800～1250 ℃ of temperature with the gypsum die body.
2. the preparation method of anode supporter of tubular solid oxide fuel cell according to claim 1 is characterized in that also comprising behind the gypsum slurry that described step a obtains adding 0.01～0.1wt% defoamer.
3. the preparation method of anode supporter of tubular solid oxide fuel cell according to claim 2 is characterized in that described defoamer is absolute alcohol or pyridine.
4. the preparation method of anode supporter of tubular solid oxide fuel cell according to claim 1 is characterized in that described step (2) is to use dropper that the anode slurry for preparing in (1) is injected the plaster mold cavity.
5. the preparation method of anode supporter of tubular solid oxide fuel cell according to claim 1 is characterized in that described metal die is cylindrical, and bottom center has detachable conical papilla.
6. the preparation method of anode supporter of tubular solid oxide fuel cell according to claim 1 is characterized in that described pre-burning is pre-burning in muffle furnace.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101834296A (en) * | 2010-06-03 | 2010-09-15 | 哈尔滨工业大学 | Method for preparing anode/electrolyte double-layer structure of solid oxide fuel cell by single grouting |
| CN101847734A (en) * | 2010-05-22 | 2010-09-29 | 东方电气集团东方汽轮机有限公司 | Method for preparing tubular solid oxide fuel cell |
| CN101306954B (en) * | 2008-07-01 | 2011-09-07 | 华南理工大学 | Method for preparing porous ceramic support |
| CN102208656A (en) * | 2011-04-30 | 2011-10-05 | 景德镇陶瓷学院 | Anode of fibrous nickel oxide-based SOFC (Solid Oxide Fuel Cell) and preparation method thereof |
| CN102306817A (en) * | 2011-08-09 | 2012-01-04 | 华南理工大学 | Method for manufacturing U-shaped hollow fiber solid oxide fuel cell |
| CN102332592A (en) * | 2011-08-09 | 2012-01-25 | 华南理工大学 | Preparation method for asymmetric hollow fiber type solid oxide fuel cell |
| CN103165903A (en) * | 2011-12-15 | 2013-06-19 | 江苏超洁绿色能源科技有限公司 | Anti-carbon-deposition, high-performance and functionally-graded anode composite film of solid oxide fuel cells and preparation method thereof |
| CN103280592A (en) * | 2013-06-07 | 2013-09-04 | 苏州诺信创新能源有限公司 | Solid oxide fuel cell combination |
| CN102292858B (en) * | 2008-12-19 | 2014-11-12 | 圣戈本陶瓷及塑料股份有限公司 | Reduction-oxidation-tolerant electrodes for solid oxide fuel cells |
| CN104803678A (en) * | 2015-04-14 | 2015-07-29 | 上海大学 | Method for preparing yttria-stabilized zirconia tubes used as SOMs (solid oxygen-ion membranes) with grouting method |
| CN105801082A (en) * | 2016-03-08 | 2016-07-27 | 安徽省大吕精机有限公司 | Fastening mould and production method thereof |
| CN105801139A (en) * | 2016-03-08 | 2016-07-27 | 安徽省大吕精机有限公司 | Smooth mould and manufacturing method thereof |
| CN106207221A (en) * | 2016-08-11 | 2016-12-07 | 山西大学 | A kind of method preparing tubular solid oxide fuel cell |
| CN106784882A (en) * | 2017-03-10 | 2017-05-31 | 佛山索弗克氢能源有限公司 | The preparation method of the anode support tube of fuel cell |
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| CN102292858B (en) * | 2008-12-19 | 2014-11-12 | 圣戈本陶瓷及塑料股份有限公司 | Reduction-oxidation-tolerant electrodes for solid oxide fuel cells |
| CN101847734A (en) * | 2010-05-22 | 2010-09-29 | 东方电气集团东方汽轮机有限公司 | Method for preparing tubular solid oxide fuel cell |
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| CN101834296B (en) * | 2010-06-03 | 2012-09-05 | 哈尔滨工业大学 | Method for preparing anode/electrolyte double-layer structure of solid oxide fuel cell by single grouting |
| CN101834296A (en) * | 2010-06-03 | 2010-09-15 | 哈尔滨工业大学 | Method for preparing anode/electrolyte double-layer structure of solid oxide fuel cell by single grouting |
| CN102208656A (en) * | 2011-04-30 | 2011-10-05 | 景德镇陶瓷学院 | Anode of fibrous nickel oxide-based SOFC (Solid Oxide Fuel Cell) and preparation method thereof |
| CN102306817B (en) * | 2011-08-09 | 2013-12-11 | 华南理工大学 | Method for manufacturing U-shaped hollow fiber solid oxide fuel cell |
| CN102332592A (en) * | 2011-08-09 | 2012-01-25 | 华南理工大学 | Preparation method for asymmetric hollow fiber type solid oxide fuel cell |
| CN102306817A (en) * | 2011-08-09 | 2012-01-04 | 华南理工大学 | Method for manufacturing U-shaped hollow fiber solid oxide fuel cell |
| CN103165903A (en) * | 2011-12-15 | 2013-06-19 | 江苏超洁绿色能源科技有限公司 | Anti-carbon-deposition, high-performance and functionally-graded anode composite film of solid oxide fuel cells and preparation method thereof |
| CN103280592A (en) * | 2013-06-07 | 2013-09-04 | 苏州诺信创新能源有限公司 | Solid oxide fuel cell combination |
| CN104803678A (en) * | 2015-04-14 | 2015-07-29 | 上海大学 | Method for preparing yttria-stabilized zirconia tubes used as SOMs (solid oxygen-ion membranes) with grouting method |
| CN105801082A (en) * | 2016-03-08 | 2016-07-27 | 安徽省大吕精机有限公司 | Fastening mould and production method thereof |
| CN105801139A (en) * | 2016-03-08 | 2016-07-27 | 安徽省大吕精机有限公司 | Smooth mould and manufacturing method thereof |
| CN106207221A (en) * | 2016-08-11 | 2016-12-07 | 山西大学 | A kind of method preparing tubular solid oxide fuel cell |
| CN106207221B (en) * | 2016-08-11 | 2018-10-26 | 山西大学 | A method of preparing tubular solid oxide fuel cell |
| CN108113875A (en) * | 2016-11-29 | 2018-06-05 | 湖南中医药大学 | A kind of multi-functional moxa cone producing device |
| CN106784882A (en) * | 2017-03-10 | 2017-05-31 | 佛山索弗克氢能源有限公司 | The preparation method of the anode support tube of fuel cell |
| CN106784882B (en) * | 2017-03-10 | 2019-05-14 | 佛山索弗克氢能源有限公司 | The preparation method of the anode support tube of fuel cell |
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